Abrasion resistant wash-wear cellulosic products



United States Patent US. Cl. 2-243 12 Claims ABSTRACT OF THE DISCLOSURECellulosic fibers are impregnated with an aqueous solution of a catalystand a thermosetting resin which may include a thermoplastic resin anddried at a temperature low enough to inhibit resin curing. Such fibersare then blended with untreated cellulosic fibers and, subsequent toforming (1) a yarn from said blend, (2) a fabric from said yarn or (3) agarment from said fabric, heated at elevated temperatures to promoteresin curing.

A non-exclusive, irrevocable, royalty-free license in the inventionherein described, throughout the world for all purposes of the UnitedStates Government, with the power to grant sublicenses for suchpurposes, is hereby granted to the Government of the United States ofAmerica.

This invention relates to a method for producing resilient textileproducts and to the products so produced. More specifically, theinvention deals with a method for producing resilient, wash-wear typecellulosic textile products from yarns composed of blends ofpartiallymodified cellulosic fibers and untreated fibers and havingexcellent fiber-and-yarn mobility. Still more specifically, theinvention deals with a novel process for the preparation of thesepartially-modified cellulosic yarns having fiber mobility from cotton(staple) fibers. When these partially-modified cellulosic yarns areconverted into fabrics or other products and subsequently exposed to ahightemperature cure, the resultant resilient products are characterizedby excellent abrasion resistance, while retaining unimpairedcrease-retention, wrinkle-resistance, and smooth-drying properties.

As used herein, the term textile products includes fabrics and articlesmanufactured from fabrics such as blouses, dresses, shorts, shirts,trousers, curtains, draperies, and the like.

The term partially-modified cellulosic yarns relates to a cellulosicyarn spun from blends of fibers and/or filaments, a portion of whichblend has been partially treated in the fiber form with a delayed-cure,crosslinking agent and the remaining portion is untreated. The resultantspun yarn comprises from about to 90 weight percent of thepartially-treated product on the total weight of the yarn. By partialtreatment is meant that the cotton fibers or other cellulosic fibershave been treated with an aqueous solution of a crosslinking agent and acatalyst for the crosslinking agent in such a manner that the curingstep which is carried out at high temperatures to complete crosslinkinis delayed. The yarns may be either singles or plied.

It is a prime object of this invention to treat cellulosic fibers withdelayed-cure, crosslinking agents and, without curing the crosslinkingagent, to process blends of the 3,483,570 Patented Dec. 16, 1969 treatedfibers with untreated cellulosic fibers into yarns which, after curing,retain excellent fiber mobility.

It is a further object to convert these yarns having excellent fibermobility, into delayed-cure fabrics which, upon subsequent curing, havesatisfactory wash-wear properties, fiber-and-yarn mobility andunexpectedly high resistance to abrasion.

It is a still further object to convert the delayed-cure fabrics havinglatent fiber-and-yarn mobility into garments or other cellulosicproducts prior to curing the crosslinking agent. The resultant curedproducts have excellent resiliency, crease-retention, shape-holding, andwash-wear properties. Most important, the retained fiber-and-yarnmobility of the cured fabrics, or garments, imparts high resistance toabrasion.

Heretofore, cellulosic textile fabrics have been treated to producewash-wear finishes by immersing the entire fabric in an aqueous solutioncomprising a suitable crosslinking agent and a catalyst to activate thecrosslinking agent, removing the excess aqueous solution by squeezingbetween padder rolls or by centrifuging, drying the wet fabric, andsubsequently curing the dry fabric to complete the crosslinking reactionbetween the agent (usually a synthetic resin) and the cellulosemolecule. During this treatment the wash-wear finish penetrates theentire fabric and also into the interior of the fibers or filaments ofwhich the fabric is composed. As a result, the fabric impregnated with awash-wear finish has greatly reduced abrasion resistance. Consequently,when these conventionally processed wash-wear fabrics are made intogarments such as dresses, shirts, blouses, shorts, trousers, and thelike, the fabrics soon show excessive abrasion at the collars, knees,creases, cuffs, and at other areas exposed to wear. The

reduced abrasion resistance as compared with noncrosslinked cellulosicmaterials is due largely to crosslinked cellulose in the fibers locatedat the fabric surface, which eliminates the ability of the fibers and/oryarns to move. More recently, wash-wear fabrics have been made intogarments, especially mens trousers, through the use of delay-curedprocesses, and these garments exhibit sharp durable creases as well asWrinkle-resistance and smoothdrying properties. However, trousers ofthis type fabricated predominantly from cellulosic fibers exhibit verypoor resistance to abrasion. Small holes, in some instances, are abradedin the cuffs and creases by merely laundering and tumble drying thegarment a few times. This has caused many textile finishers to usefabrics containing a blend of noncellulosic and cellulosic fibers in aneffort to overcome the loss in abrasion resistance after resintreatment. The use of these blends has caused a substantial increase inthe cost of wash-wear fabrics.

We have now discovered that wrinkle-resistant, smoothdrying fabricscontaining durable creases, good shapeholding properties, and excellentabrasion resistance can be produced in a remarkably simple andunexpected manner by treating staple cotton fibers (frequently referredto herein as fibers) with a crosslinking agent, but without curing theagent, and thereafter blending the dry, treated fibers with untreatedcotton fibers. The blend is then carded, drawn, and spun into yarn. Theyarn may then be cured, or, without curing, it may be Woven intofabrics, after which the uncured crosslinking agent (resin) is cured byheat treatment at elevated temperatures. Or, the uncured fabric may beconverted into garments or other commercial products which may becreased in selected locations and hot pressed, after which thecrosslinking agent is cured by exposure to high temperatures for asuitable time. The resultant cured yarns, fabrics, or garments arecomposed of a blend of modified (crosslinked) and unmodified fibers,retain excellent fiber-and-yarn mobility, and a high degree ofresistance to abrasive damage such as is encountered in home-typewashing machines and tumble dryers.

In general, the process of our invention may be described as follows:

(a) Opened cotton fibers, preferentially cotton fibers that have beenscoured and bleached, are fed (passed) ,by suitable means into atreating bath comprising an aqueous solution of a synthetic resin(crosslinking or treating agent) and a catalyst for said resin;

(b) A period of dwell (residence time) is then maintained to permit theaqueous solution to wet the fibers;

(c) The excess aqueous solution is then removed .to give a wet pickup ofabout 85 to 110 weight percent on the weight of the fibers (OWF);

(d) The wet fibers are then dried at a temperature not over 200 F. to amoisture content of not less than weight percent;

(e) The dried fibers are then permitted to equilibrate at ambient roomtemperature and humidity to reduce the moisture further to about 5.5 to8.0 weight percent of the total weight of the fiber and the depositedresin (chemical). This may require from about to 24 hours.

(f) The resin treated and equilibrated fibers are then blended withuntreated cellulosic fibers;

(g) The blends are then converted into yarns of a predetermined size andtwist by the conventional processing steps for converting cotton fibersinto yarns;

(h) The yarns are then crosslinked, or cured, by heating them at atemperature from about 240 F. to 350 F. for about to 3 minutes wherebyresilient yarns having excellent fiber mobility and capable of producingresistance to abrasion are obtained.

(i) In another embodiment of this invention, the blended yarns of step(g), without curing, may be woven into a fabric after which the fabricmay be exposed to elevated temperatures of about 240 to 350 F. forappropriate periods of time to cure or effect crosslinking. About 3 to 8minutes at about 325 F. is a good practice.

(i) In still another embodiment of our invention, the uncured fabric isconverted into garments, creased, pressed, or otherwise physicallyaltered at selected locations by means of hot-pressing or other meansknown to those skilled in the art, after which the garment is cured byexposure to similar high temperatures for appropriate periods of time toeffect crosslinking of the thermosetting or thermoplastic resins.

The process is simple and easily applied. The cellulose fibers may betreated by conventional means known to those skilled in the art. Aftertreatment, the equilibrated uncured staple fibers are blended withunscoured; or scoured; or scoured and bleached cellulosic fibers invarying amounts and processed into yarns, fabrics, and other cellulosicproducts (such as garments, knit goods, curtains, draperies, etc.,) byconventional cotton processing equipment, or equipment required tofabricate the other products. Due to the presence of the potential(latent) properties of crosslinking ability with the cellulose molecule,and the application of these agents prior to any mechanical operationsdirected at making yarns or fabrics, these yarns, fabrics, and garmentsafter curing retain a high degree of fiber-and-yarn mobility and alsoexcellent properties of Wrinkle-resistance, smooth-drying,durablecreasing, and good shape-holding. Most important, the resultantproducts are characterized by excellent resistance to abrasion.

Preparation of aqueous solutions of treating agents Crosslinking agentssuitable for use in the practice of our invention include reagents thatcontain two or more functional groups that are capable of reacting withthe cellulose or with themselves. Two types of crosslinking agents havecaused excellent results to be obtained, namely, essentially monomericthermosetting crosslinking agents and essentially monomericthermoplastic crosslinking agents. As will be more fully explained inthe examples, either the warp yarns, the filling yarns, or both warp andfilling yarns may be spun from blends of the treated and untreatedfibers.

Typical examples of essentially monomeric, commercially availablethermosetting crosslinking agents are N,N'- dimethylol-4,5-dihydroxycyclic ethylenurea, dimethylol hydroxyethyl carbamate',bis-methoxymethyl ethylcarbamate, vinyl cyclohexene-diepoxide, acetals,and related crosslinking agents that have a slow rate of cure (longshelf life) under ambient conditions of temperature and humidity.Typical examples of essentially monomeric, thermoplastic crosslinkingagents are the commercially available vinyl acrylic resins,self-crosslinking acrylic resins, vinylidine chloride modified acrylics,styrene-butadiene resins, vinyl acetates,butadiene-acrylonitrile-styrene terpolymers, styrene-methylolpolyamidecopolymers, vinylmethylolpolyamide copolymers, acrylo-methylolpolyamidecopolymers, and the like. Although these latter resins are designated ascopolymers or terpolymers, they are essentially monomeric and capable ofcrosslinking and form a thin tough film around the fiber.

The self-crosslinking acrylics do not crosslink to any appreciableextent until they are cured at a temperature over 240 F. Until thistime, the resins exhibit thermoplastic behavior. After curing, theacrylic resin exhibits both thermosetting and thermoplastic properties.The better the cure, the greater the number of crosslinks and the morethe properties of this type of resin resemble those of a thermosettingresin. The cure can be made on the yarn, or the fabric; or the fabricmay be converted into garments and then cured. As noted above, theseresins form a thin, tough film around the individual fibers.

Regardless of the type used, the concentration of the crosslinking agentin the treating bath should be adequate to deposit from about 1 to 20weight percent dry resin add'on after the fibers have been dried andequilibrated. Usually, concentrations of about 1 to 20 weight percent onthe weight of the solution (OWS) with a subsequent wet pickup of aboutto weight percent on the weight of the fiber (OWF) is a good practice.

Catalysts suitable in this invention are those commonly used with thecrosslinking agents of the types listed above. For the thermosettingresins, typical examples include zinc nitrate, zinc fluoroborate,solutions of zinc salts buffered with organic acids such as acetic acid,magnesium chloride, and metallic salt complexes containing Zinc. For thethermoplastic resins, typical examples include oxalic acid, magnesiumchloride, Z-amino-Z-methyl-l-proponal hydrochloride, zinc nitrate, andsimilar acid or latent acid catalysts. Latent acid catalysts refer toproducts which become effective at curing temperatures. However, inorder to be suitable for the practice of the present invention, thesecatalysts must be neutralized, or buffered, where necessary, so that theaqueous crosslinking solution containing the catalysts is neutral orslightly acidic. In general, it is preferred that the pH of the aqueouscrosslinking solution be in the pH of the aqueous crosslinking solutionto be in the range of 3 to 7. Low pHs, i.e., about 2 or lower, are notsuitable because of the increased susceptibility of the crosslinked,uncured fibers to cure during the subsequent conventional cottonprocessing or storage. Also, there is a potential danger ofacid-tendering of the treated fibers. Alkaline pHs, i.e., above 7, arelikewise unsuitable. Use of alkaline pad baths results in reducedefficiency of the crosslinking reaction, produces yellowing of the yarnsand/or fabric upon heating, and reduce the quality of durability ofwash-wear properties and creases imparted to the cellulosic product. Aparticularly suitable pH range for the aqueous crosslinking solution ofthe present invention is 5 to 7, preferably 56.5. The adjustment of thepH of the latent acidforming catalysts, zinc nitrate, and magnesiumchloride, to produce the aqueous crosslinking solution having a pH of6.5 or slightly lower may be accomplished by the addition of anycompatible alkaline agent or by the use of bufiers. The zinc nitratecatalyst should not be buffered or neutralized to above a pH of 6.5 toavoid precipitation of water-insoluble, noncatalytic zinc hydroxide.Should this precipitate appear, addition of a few drops of acetic acidis usually sufficient to reduce the pH of the aqueous crosslinkingsolution to a pH below 6.5 and prevent the formation of zinc hydroxide.

The amount of catalyst employed will depend upon the amount ofcrosslinking agent. However, amounts ranging from about 0.5 to 5 weightpercent (OWS) is a good practice for the thermosetting crosslinkingagents. Amounts ranging from about 0.1 to 2.0 weight percent (OWS) causesatisfactory results to be obtained with the thermoplastic resins. Theself-crosslinking acrylics do not require an additional catalyst, but asnoted above, require a cure for crosslinking to occur. The particularcatalyst to be used With a particular crosslinking agent is known tothose skilled in the art.

Auxiliary agents suitable for use in this invention are softeners,wetting agents, optical whiteners, dyes, lower alkyl alcohols, such asethyl and isopropyl alcohols, methyl ethyl ketone, dimethyl formamide,and other commonly used finish modifiers. The reactive dyes discussed inthe examples serve to color the fibers and also serve to identify thepercentage add-on, thus simplifying the blending of the treated fibershaving varying types of resins or different add-ons.

A typical example useful in the practice of this invention comprises 12weight percent dimethylol dihydroxy ethyleneurea, 0.2 weight percentwetting agent, 1.0 weight percent dye, 3.0 weight percent alcohol methylethyl ketone, dimethyl formamide, and the like, and the balance water,all percentages (OWS).

Typical wetting agents are ethyl, methyl, and isopropyl alcohols;nonionic agents such as alkylaryl polyether alcohols, alkylarylpolyglycols, and the like.

Typical dyes are optical whiteners, and reactive dyes such as ReactiveRed 12, Reactive Violet 2, Reactive Yellow 6, Reactive Blue 5, and thelike.

Typical softening agents are polyethylene, polypropylene, and thenonionic fatty ester-amides. These auxiliary agents are not limitingfeatures of this invention.

Treating the cotton fibers Cotton fibers, preferably scoured andbleached, are passed into, and through, the aqueous bath comprising thetreating agent and catalyst. The fibers may be in form of a picker-lapenclosed (encased) in scoured and bleached cotton gauze. The gauze tendsto hold the lap in position and simplifies the treating operation. Weprefer the use of a 13 oz./yd. picker-lap, encased in scoured andbleached 20 x 24 count cotton gauze but this method is not a limitingfeature of this invention.

A period of dwell (residence time) in the aqueous treating bath ismaintained for sufiicient time to permit the aqueous solution to wet,and for the thermosetting resins to penetrate, the individual fibers.Excess treating solution is then removed by use of a centrifuge, orpadder rolls. We prefer the latter. It is a critical feature of ourinvention that the fi'bers have a wet pickup of about 85 to 110 Weightpercent (OWF) of the aqueous crosslinking solution, and it is within thescope of our invention to give the fibers more than one pass through theaqueous treating bath and squeeze rolls to ensure that the proper pickupis achieved.

When the cellulosic fibers are unscoured, the use of one or more of thewetting agents listed above aids in reducing the time required forwetting and/or penetrating the fibers by the aqueous solution. However,for scoured, or

6 scoured and bleached cellulosic fibers wetting agents are not criticalfeatures of this invention.

Drying the treated fibers The wet fibers are then dried. We have foundthat drying in a continuous festoon-type drying oven is a good practice.It is a critical feature of the drying step that the air temperature ofthe oven be no greater than about 200 F. to prevent prematurecrosslinking of the cellulosic material. This is particularly importantfor crosslinking agent of the thermosetting type.

It is another critical feature of this invention that the moisturecontent, during heat drying, be reduced no lower than about 10 to 12weight percent (OWF).

Equilibration The treated fibers are then equilibrated, i.e., areexposed to ambient room temperature and humidity conditions for a periodof time during which the moisture content of the treated fibers isfurther reduced to about 5.5 to 8 weight percent (OWF). Afterequilibration, the treated fibers are flexible, pliable, and may bereadily processed on the equipment used in conventional cotton systems.This equilibration step is a critical feature of this invention.Overdried fibers may, and often do, break during further processing onconventional cotton systems and the resulting yarns and/or fabrics arecommercially unacceptable. The equilibrated fibers may contain fromabout 1 to 20 weight percent (OWF) dry crosslinking agent based on thetotal weight of fiber and add-on, the exact amount depending upon theultimate end-use of the fabric into which the blends are to beprocessed.

The precedure for impregnating untreated cellulosic fibers with athermoplastic crosslinking agent is generally similar to the procedurefor the thermosetting crosslinking agents, using the suggested catalystfor the thermoplast. It is an advantage in the process of our inventionthat the aqueous solutions of the two types of resins may be appliedseparately, or applied together. As noted above, some thermoplasticcrosslinking agents do not require a catalyst.

Treatment of the cellulosic fibrous materials with aqueous solutions ofthese essentially monomeric crosslinking resins, and drying attemperatures not greater than 200 F. imparts latent crosslinkingproperties to the treated fiber, and when it is subsequently cured,either in the form of yarns, fabrics, or after the fabric has beenconverted into garments, the cured products have retained theirfiber-and-yarn mobility. These cured products show excellent resistanceto abrasion.

Blending treated and untreated fibers Three general types of blends maybe obtained: (a) blends of fibers treated with thermosetting resins anduntreated fibers; (b) blends of fibers treated with thermoplastic resinsand untreated fibers; and (c) blends of both (a) and (b) with untreatedfibers.

When only a single type of crosslinking agent is used in preparing theblend (that is, thermosetting or thermoplastic) from about 10 to weightpercent of the treated fiber may be used with about 90 to 10 weightpercent untreated fiber. This is true for treatments with boththermosetting crosslinking agents and with thermoplastic crosslinkingagents. However, it is a critical feature of the process of thisinvention that there is always a blend consisting of treated anduntreated cellulosic fibers. The presence of the untreated fibers plusfibers treated in our novel way permit fiber and yarn mobility in thecomposite yarn and/ or fabric. It is this fiber-and-yarn mobility whichimproves the resistance to abrasion of the crosslinked products made byour novel process. This mobility is present in the yarns, the fabrics,or the products made from the fabrics, during the processing steps andis retained after the curing, 0r crosslinking, step. This wasunexpected.

As noted above, it is within the scope of our invention to use fiberstreated with a thermosetting resin along with fibers treated withthermoplastic resin, and untreated fibers in the blend, the blendsubsequently to be processed into a yarn. When these three fibers (twotreated and one untreated) are used, we prefer to use at least 10 Weightpercent (OWF) of the untreated fibers. The ratio of fibers treated witha thermosetting resin to fibers treated with a thermosplastic resin mayvary from about 10 to 90 weight percent. In a typical example of a blendof this type, the yarn might contain 10 weight percent untreated fibers,and 45 weight percent of each type of treated fibers. However, theparticular ratio of the two types of treated fibers is not a limitingfeature of the present invention, good results having been obtained wheneach of the three types of fibers is present in equal amounts, circa33.3 weight percent.

When the type of blend and the desired amount of each fiber in the blendhave been determined, the next step is to process these blends intoyarns and/or fabrics.

It is also a critical feature of this invention that the particularresin employed is a delayed cure type which under ambient conditions oftemperature and pressure permits the user to defer curing untilconvenient for his purposes. Deferred or delayed cure as intended hereinmeans that the chemical reaction between the crosslinking aganet and thecellulose (for thermosetting resins) or the crosslinking between themolecules of the thermoplastic resins will not be completed in less thanone week, preferably one to six months, at ambient room temperature andhumidity.

Processing the blends It is an advantage of the process of our inventionthat the blends may be processed by conventional cotton systems.

The treated fibers in the form of a picker lap (as noted above) areformed into sandwich-type layers with untreated fibers and again passedthrough the picker, then through the card, drawing frames, rovingframes, and finally spun into yarns. They are then woven into fabrics,and when desired, given a heat treatment (or cure) at about 240 to 350F. for 20 to 3 minutes (or appropriate time intervals dependent ontemperature) to complete the crosslinking between the treating agent andthe cellulose. If, however, the fabric is to be converted into garments,or other cellulosic products, the cure is delayed until the garment, orother product has been fabricated. This will be discussed below.

It is also within the scope of our invention that the cellulosic fibersare treated in bulk form with the aqueous solution of crosslinkingagent. When this procedure is used, the treated, dried, and equilibratedfibers are fed through the picker to form a picker-lap, then formed intothe sandwich with the untreated fibers and again passed through thepicker, card, drawing frames and spun into yarns as above. These yarnsmay be cured, or the uncured yarns are then woven into fabrics and maybe cured in fabric form. Or the cure may be delayed until the garment orother cellulosic product is manufactured from the uncured fabric.

It is also within the scope of this invention to pass the treated oruntreated fibres through the card to form a card sliver of each and thenblend the two slivers at the drawing frame. Or, the treated anduntreated sliver may be blended at the drawing frame and a secondtreated fiber, in the form of card sliver, may also be blended with thefirst two at the drawing frame. The particular machine on which theblends are formed is not a limiting feature of this invention.

It is an advantage of this invention that the proportion of treatedfibers and their resin add-on can be varied at will depending upon theproperties desired in the end product. For example, 50 parts (percent)treated cotton fibers may be blended with 50 parts (percent) untreated,scoured and bleached cotton fibers at the picker. This of course gives100 parts of 50% treated and 50% untreated. In another example, 25%treated fibers may be blended with untreated fibers at the picker; or50% treated fibers may be blended with 50% untreated fibers at thepicker after which three card sliver ends of this 50-50 blend may beblended with three card sliver ends of treated fibers resulting in anoverall blend of 75% treated fibers and 25% untreated fibers; or, 50parts untreated cotton fibers may be blended with 50 parts thermosettingresin-treated fibers at the picker (a 50-50 blend) and then four ends ofthis 5050 blend is blended with two ends of 100%thermoplastic-resin-treated cotton fibers resulting in an overall blendconsisting of one-third thermoplastic-treated fibers, one-third ofthermosettingtreated fibers and one-third of untreated fibers. In any ofthe above blends, the resin add-on may range from about 1 to 20 weightpercent of the crosslinked-treated fibers. The object here is to use theparticular resin add-on and blend to produce the desired properties ofcrease retention, flat drying, resiliency, wash-wear, and greatlyincreased abrasion resistance. The above slivers (drawing slivers) arethen converted into roving, which in turn is converted into yarn usingconventional cotton procedures. The yarns may then be cured, or theuncured yarns may be woven or knitted into fabrics and cured. Or theuncured fabrics may be converted into garments and the like, preformedby molding or creasing as desired, after which the preformed product iscured. The resultant cured product retains its formed shape. The weavingor knitting involves no deviation from normal weaving or knittingprocedures.

The process is simple and easily applied, and very little, if any,mechanical processing difficulties are encountered. The products of thisinvention have successfully withstood up to 40 home washing-tumbledrying cycles according to the procedure 88A 1964T of the AmericanAssociation of Textile Chemists and Colorists, whereas control fabricswhich were treated with the same resins by a padding technique(impregnating) to give comparable resin add-ons showed excessiveabrasion damage after less than 10 such laundering cycles. Further,fabrics containing blends of treated-untreated fibers in both warp andfilling had excellent flat drying properties, crease retention,resiliency, and showed only a minimum of abrasive damage after the 40home washing-tumble drying cycles.

The following examples are set forth by way of illustration only, and itwill be understood that the invention is not to be construed as limitedin spirit or scope by the details therein. Temperatures are given indegrees Fahrenheit unless otherwise noted. All parts are percentages areby weight. Test results are according to standard test methods asdesignated by the American Association of Textile Chemists and Colorists(AATCC) or the American Society for Testing Materials (ASTM). Thecrosslinking agent is frequently referred to below as the chemical orsynthetic resin.

Wash-tumble dry: AATCC Test Method 88A-1964T Flex abrasion: ASTM TestMethod D 1175-64T Flat abrasion: ASTM Test Method D 1175-64T Tearingstrength: ASTM Test Method D 1424-63 Wrinkle recovery: ASTM Test MethodD 1295-60T Example 1 The following example illustrates the effect ofdifferent levels of thermosetting resin add-on on the performance ofcotton garments with regard to flat drying properties, crease retention,and resistance to abrasion.

(A) As the starting material, commercially scoured and bleached mediumstaple cotton fibers are used. These fibers are processed into 13oz./yd. picker lap, and for ease of handling for chemical processing,the lap is encased in scoured and bleached 20 x 24 count cotton gauze.

(B) Three treating solutions are prepared using as the crosslinkingagent dimethylol dihydroxy-ethylene urea.

All ingredients are parts by weight based on the total weight of thesolution.

Ethyl alcohl Reactive Red 12. Reactive Yellow Reactive Blue ReactiveBlue 5 Water to 100 parts.

1 Metallic salt complex containing zinc stabilized with acetic acid. 3Trimethyl nonyl ether of polyethylene glycol.

(C) The encased picker laps from (A) above are fed into a laboratorypadder containing the solutions described in (B) above at the rate ofabout 0.75 yard per minute and passed twice (two dips and two nips) intoand through the aqueous solution of crosslinking agent over a 2.3 minuteperiod of time. A wet pickup of 95% is achieved from the and the 20%solids solutions, and a wet pickup of 86% from the 14% solids solution.The padded cotton is then dried in a continuous festoontype drying ovenat a temperature not exceeding 200 F., with care being taken to dry thetreated cotton to about 10-12% moisture. The balance of the water isthen removed by equilibration overnight (about 15 hours). Afterequilibration, the treated samples contain 8.8% dry chemical add-on,12.1% dry chemical add-on, and 18.1% dry chemicall add-on, respectively.

(D) Portions of the equilibrated but uncured treated cotton fibers from(C) above, still in lap form, are then sandwich-blended with (1) anequal weight of scoured and bleached fibers also in lap form, and (2)one-third of their weight of scoured and bleached fibers in lap form,then processed through a picker to produce picker laps of about 13.7ounces per yard. The lap containing 50-50% treated-untreated fibers, andthe lap containing 75-25% treated-untreated fibers, and a control lapcontaining only scoured and bleached untreated fibers, are thenindividually processed on a Crosrol-Varga metallic card at a cylinderspeed of 240 r.p.m., a lickerin speed of 600 r.p.m., and a productionrate of 10 pounds per hour in the form of 47.0 grains/ yard sliver. Ablend containing 25% treated and 75% untreated fibers is made by feedingthree ends of the 5050% sliver and three ends of the untreated fibersliver to the drawing frame. Each lot is drawn twice, with the finalproduct being 45 grains/ yard second drawing sliver. A 3.8 hank rovinghaving a 1.3 twist multiple (TM) is then produced and spun into 30/ 1yarn using a 3.5 TM. These yarns are then woven into a 64 x 112 fillingface sateen using a starch sized warp of untreated, unscoured, andunbleached cotton fibers. The ratio of filling weight to Warp weight is1.75 to 1 for all sateens.

(E) Simulated trouser cuffs are then made from the fabrics produced in Dabove with the crease for the trouser cuff in one case running in thewarp direction, and in the other in the filling direction. Afterfabrication, the trouser cuffs are cured for 10 minutes at 320 F.(delayed-cure) after having been hand ironed to flatness and to insertthe leg creases. The trouser cuffs are then evaluated for theirresistance to abrasion by subjecting them to 60 wash-wear launderings,each loundering consisting of one Washing and one drying cycle. The washcycle in a home-type washer lasts seven minutes and is followed by acold rinse, a warm rinse, and a spin-dry cycle using AATCC Test Method88A-1964T with an 8-pound load. Soap used is 75 cc. of detergent (Tide)with a high-water setting (17 gallons). The drying cycle is 65 minutesin a home-type, electrically-heated tumble dryer. Both the washer anddryer meet the American Association of Textile Chemists and Coloristsrequirements for wash-tumble dry evaluation of resin-treated fabrics orgarments.

(F) the simulated trouser legs are then examined after 2, 5, 8, 10, 12,15, 18, 20, 23, 25, 28, 30, 33, 35, 38, 40, 43, 45, 48, 50, 55, and 60launderings. Trouser creases are best when made parallel to warpdirection on the fabric, and cuff creases best when trouser leg is madeparallel to the filling direction. In each of these two cases, thebetter results are to be expected because the creases are actually beingplaced in the treated fibers of the filling yarn and not in theuntreated warp yarn. As the chemical (resin) add-on of the treated fiberfraction increases, the abrasion due to washing and drying tends toincrease, particularly Where the percentage of treated fibers in thefilling is high. Flat drying properties are improved with increasingchemical add-on. In no case is any abrasion damage noted before 35Wash-dry cycles, and at the 8.8% chemical add-on level for the treatedfibers only some suspicious spots are evident after 60 laundry cycles.At the 18.1% chemical or resin add-on level, all samples demonstrateprogressively increasing abrasive wear from 35 through 60 cycles oflaundering, Wltil some crease wear evident after 48 laundry cycles. Ingeneral, we found that a chemical add-on of about 12% in 50% of thefilling fibers (4.53 weight percent resin add-on by nitrogen analysis onthe total weight of the fabric) result in a product that has the bestWashwear characteristics of crease retention, fiat drying, andresistance to abrasive damage during washing and tumble drying.

EXAMPLE 2 Bath N0. 1 Bath N0. 2

Bath No. 3

Wetting agent 2 Ethyl alcohol.

Reactive Red 12 Reactive Yellow 6 Reactive Blue 5 Reactive Blue 5 1Metallic salt complex containing zine stablized with acetic acid. 2Trimethyl nonyl ether of polyethylene glycol.

(C) The encased picker laps from (A) above are impregnated in theaqueous solution using alaboratoryscale padder and the procedure ofExample 1. The impregnated cotton is then dried in a continuousfestoontype drying oven at a temperature of 200 F. with a resideuce timeof 25 minutes. Moisture content of the dried cotton is held to a 10%minimum. The treated products are then equilibrated overnight. Afterequilibration, the samples show a 7.0% dry resin add-0n, a 12.1% dryresin add-on, and an 18.1% dry resin add-on, respectively, whichindicates that the wet add-on of chemical treating solution variesbetween 86 and for these three treatments.

(D) Portions of the equilibrated but not cured treated cotton fibersfrom (C) above and still in lap form are sandwich-blended with (1) anequal weight of untreated, scoured, and bleached fibers also in lap formon the apron of the picker and processed into a 13.7 oz./yd. blendedpicker lap containing 50% treated and 50% untreated fibers at each ofthe three levels of crosslinking chemical add-on; and (2) one-third oftheir weight of untreated, scoured, and bleached fibers in picker-lapform on the apron of the picker and processed into 13.7 oz./yd. pickerlaps containing 75% treated fibers and 25% untreated fibers at each ofthe three levels of chemical add-on. The lots of each treatment at eachof the three chemical addon levels and the two blending levels are thencarded on a Crosrol-Varga metallic card at a cylinder speed of 240r.p.m., a lickerin speed of 600 r.p.m., and a production rate of poundsper hour in the form of 47.0 grains per yard sliver. A lap of thecontrol scoured and bleached fibers is also processed through theCrosrol-Varga card under the same conditions as the laps containingblanded amounts of treated and untreated fibres. Each of these lots offibers are then drawn twice using six ends of sliver each time and adrawing sliver of 45 grains/yd. is produced. A blended sliver containing25% treated fibers and 75% untreated fibers is produced by feeding threeends of the 5050% blend and three ends of the untreated, scoured, andbleached sliver to the drawing frame. After the second drawing, a sliverof 45.2 grains/yd. is produced. Each of these lots of blended sliver areprocessed into 3.8 hank roving having a 1.3 TM, and then spun into 30/1yarns using a 3.5 TM, and the resulting yarns are woven into a 64 x 112filling face sateen using a starch sized warp which consists ofuntreated, unscoured, unbleached cotton fibers.

(E) Simulated trouser legs and cuffs are then made from the fabrics from(D) above with the pattern so placed that two trouser legs are cut inthe warp direction, and two in the filling direction from eachexperimental fabric. After fabrication into these simulated trouser legsand cuffs, the samples are ironed using a hand electric iron, set at thecotton setting, into flat surfaces, and creases are placed at thedesired points. The pressed or ironed samples are then cured at 320 F.for 10 minutes. The cured simulated trouser legs with cuffs areevaluated for their resistance to abrasion by subjecting them to 60wash-wear washing-and-drying cycles using home-type washing and dryingequipment. This procedure and wash cycle and drying cycle are identicalwith those described in Example 1.

(F) The simulated trouser legs were examined at the same intervals as inExample 1. It was observed that the flat drying properties increase withincreasing amounts of treated fibers present, and that the pilling ofthe fabric decreases with increasing amounts of treated fibers. Creaseretention improves with increasing amounts of treated fibers. Creases inthe leg portion of the trouser are best when the pattern is cut so thatthe creases are parallel with the warp of the fabric. Cuff creaseretention and appearance is best when the pattern is cut so that thecreases and flat surfaces are made parallel to the filling direction ofthe fabric. In these two cases, this phenomena would be expected sincethe warp is untreated and contributes little to either fiat-dryingproperties or to the creaseretention characteristics of the fabrics. Inno case is significant abrasion damage due to washing and drying notedbefore 35 wash-dry cycles, and then only at the lowest and intermediatelevels of blends, i.e., those containing 25% and 50% treated fibers,respectively. When the treated fiber content is 75 in the filling, allsamples demonstrated some abrasive damage, progressively increasing from35 through 60 cycles with some crease-wear evident after 48 cycles whenthe chemical add-on is 18.1% in the treated fraction of the fibers, withsubstantially less evident abrasive deterioration at the 50% treatedfiber fraction and below. In general, where the chemical add-on is about12%, and the treated fraction of the fibers amounts to 50%, the productperformance is best in terms of flat drying characteristics, resistanceto pilling, crease retention, and reduced abrasion damage duringmultiple wash-dry cycles of simulated usage.

When the above example is repeated using dimethylol hydroxyethylcarbamate, or bismethoxymethyl ethyl carba-mage, or vinyl cyclo hexenediepoxide instead of the dimethylol dihydroxy cyclic ethyleneurea,generally similar results are obtained.

12 Example 3 This example illustrates the beneficial effects of havingboth thermoplastic and thermosetting resinous treatments on separatefractions of the fibers going into blends to improve product performancein such characteristics as flat drying, crease retention, and resistanceto abrasion such as occurs during washing and drying using hometypelaundry equipment.

(A) Portions of the same scoured and bleached rawstock cotton fibersused in Example 1 are used and processed as in Example 1.

(B) A treating solution is prepared using a thermoplasticself-crosslinking acrylic resin as follows:

Bath No. 1 Self-crosslinking acrylic resin 1 10.0 Wetting agent 2 0.2Ethyl alcohol 3.0 Reactive Yellow 6 1.0

Water to parts.

1 Aqueous acrylic dispersion of thermoplastic resin-HA-20 sold by Rohm &Haas.

2 Trimethyl nonly ether of polyethylene glycol.

(C) The crosslinking chemical is applied to the cellulosic fiber by theprocedure of Example 1 using a laboratory-scale padder with two dips andtwo nips with the feed rate set at 0.75 yd. per minute, and a residencetime (period of dwell) in the padder of 2.3 minutes. From the padder thetreated picker lap is fed into a festoon type continuous dryer and heldat 200 F. for approximately 25 minutes. After equilibrating overnight,the treated fiber analyzes 2.8% acrylic resin add-on by the method ofKanter and Hoey, American Dyestuff Reptr. 52 (14) 515516, July 8, 1963.

(D) Because some adherence between fibers is observed after the acrylictreated fibers are equilibrated overnight they are then passed through alaboratory-scale cotton opener, through a willow, a downstroke, a secondopener, and thence into the picker to be formed into 16 oz./yd. lapwhich is then carded on the Crosrol-Varga metallic card into 47grain/yd. sliver. Two ends of this sliver are then fed into the drawingframe along with four ends of the blend containing 50% of fibers treatedwith an 8.8% add-on of dimethylol dihydroxy ethyleneurea (fibers fromBath A--Example 1) and then drawn twice to produce a 45 grain/yd.second-drawing sliver which consists of 33.3% fibers treated withdimethylol dihydroxy ethyleneurea at the 8.8% add-on level, 33.3% fiberstreated with the self-crosslinking acrylic dispersion at the 2.8% level,and 33.3% untreated, scoured, and bleached fibers. Similar proceduresare used in the production of blends in sliver form consisting of 33.3%dimethylol dihydroxy ethyleneurea treated fibers at the 12.1 and at 18.1levels (Baths B and C of Example 1) with 33.3% of the acrylic treatedfibers and 33.3% untreated scoured and bleached fibers, and theresulting sliver weighs 45 grains per yard. These slivers are thenprocessed into 3.8 hank roving using a 1.3 TM, then into 30/1 yarns with3.5 TM, and then woven into a 64 x 112 filling face sateen using astarch sized warp of untreated, unscoured, and unbleached cotton fibers.

(E) Simulated trouser legs and cuffs are then made from fabrics from (D)above with the pattern so placed that two samples may be cut in the warpdirection of each fabric, and two in the filling direction of eachfabric. After the simulated garments are made they are hand ironed witha home-type electric iron set at the cotton setting to obtain flatsurfaces and creases where desired. Following ironing the samples arecured at 320 F. for 10 minutes. (As noted above, the self-crosslinkingacrylics require a cure at temperatures of at least 240 F.) The curedsimulated trouser legs and cuffs are then evaluated for their resistanceto abrasion such as occurs in laundering by subjecting them to 60wash-wear cycles of washing followed by tumble drying in a home-typewasher and 13 dryer. The procedure and drying time temperatures ofExample 1 are followed.

(F) The samples were examined visually for signs of abrasion damage atthe same intervals as described for Example 1. We found that thepresence of the thermoplastic treated fibers in the yarns significantlyimproved the appearance and the resistance of the samples to abrasiondamage during washing. None of the samples containing the thermoplastictreated fibers in addition to the thermosetting treated fibers exhibitedany abrasion damage either in the cuff area or in the creases, after thesamples had been subjected to 60 wash-dry cycles. As previously observedin Examples 1 and 2, the creases in the leg portion of the samples areconsiderably better when the pattern is cut so that these creases fallparallel to the warp than when the pattern is cut so that the creasesare parallel to the filling. The obvious explanation for thisobservation is that when the creases are parallel to the warp, thetreated fibers in the filling yarns are being creased; and when thecrease is parallal to the filling, untreated fibers are being creasedsince the warp yarns are untreated. The opposite should hold for thecuffs due to the direction in which they are folded at 90 to the creasein the trouser leg. This, too, is confirmed by direct observation of thesamples. Improved flat drying characteristics and improved creaseappearance accompanied the increase in the thermosetting chemicaladd-on, although there is an indication that very satisfactoryperformance in these two properties can be obtained at add-ons as low as8.8% in the thermosetting treated fiber part of the blend. This resultsthen in the average add-on for the fabric expressed in terms ofthermosetting resin of 1.02% and an average resin add-on in terms ofthermoplastic resin of 1.17%. Much reduced pilling is noted when thethermoplastic resin is present in the fabrics.

Example 4 This example illustrates the beneficial effects in suchproperties as flat drying, crease retention, tensile strength, andresistance to abrasion damage of having both the warp and the fillingcomposed of a blend of resin treated and untreated cotton fibers.

(A) Portions of the same scoured and bleached cotton rawstock used forExample 1 encased in gauze are processed by the mechanical procedure ofExample 1.

(B) The treating solution in this example consists of a 13% resin solidsconcentration of dimethylol dihydroxy ethyleneurea, 0.27% of alkylarylpolyglycol, 3.25% ethyl alcohol, 0.5% zinc nitrate complex catalyst, 1%Reactive Brown dye, and 81.96% water.

(C) The untreated fibers (picker lap) are then passed into, and through,the aqueous solution of (B), using the laboratory-scale padder describedin Example 1, with the same feed rate and residence time and with thewet pickup controlled to about 86%. The wet picker lap is then passedthrough the festoon type dryer under the same conditions as described inExample 1. After equilibrating overnight, the treated fibers analyzed10.4% resin content.

(D) Approximately 45 pounds of the treated lap are sandwich blended atthe apron of the picker with an equal amount of untreated but scouredand bleached cotton fibers in the form of picker lap, then processed toproduce picker laps of about 13.5 oz. per yard. Similarly, about sixpounds of the treated lap are sandwich blended at the apron of thepicker with about two pounds of untreated, secured, and bleached pickerlap and processed into 13.6 oz. per yard picker laps which yields ablend having 75% treated and 25% untreated fibers. These two blends arethen individually carded on a (Crosrol-Varga) metallic clothed card at acylinder speed of 240 r.p.m., a lickerin speed of 600 r.p.m., and aproduction rate of pounds per hour in the form of 45 grains/ yd. sliver.

A portion (82 pounds) of the blend containing equal weights of treatedand untreated fibers in card sliver form are then drawn twice, feedingsix ends each time to assure evenmore intimate blending of the fibers inthe final drawn sliver which weighs 45 grains per yard. This isdesignated Blend A. The remaining eight pounds of the equal-weight blendof treated and untreated fibers are then reduced to a 25 treated fiberand 75 untreated fiber blend by feeding three ends of the 50% treatedfiber, 50% untreated fiber card sliver, and three ends of 45 grainsliver previously made from the scoured and bleached rawstock which hasnot been treated. These ends are fed through the drawing frame twice andthe resulting drawing sliver weighs 45 grains per yard. This isdesignated Blend B.

The blend containing 75 treated fibers and 25 untreated fibers is drawntwice, feeding six ends on each pass to the drawing frame. The resultingsliver weighs 45 grains per yard and is designated Blend C.

From each blend, roving is produced, which, in turn, is processed inseveral different ways:

(a) to produce a warp, about 75 pounds of Blend A are spun into 50/1yarns having a 4.25 TM which are doubled or plied into a 50/2 yarn,creeled and wound onto a warper reel, and thence onto a suitable warpbeam. The ends are then drawn into 10 harnesses which permit the weavingof a three up two down twill fabric.

(b) Another portion of Blend A, weighing about six pounds, is spun into13.5/1 yarn having a TM of 3.5. This is then used as filling yarn.

(c) Blend B is spun into 13.5/1 yarns having 3.5 TM and are used asfilling yarns.

(d) Blend C is spun into 13.5/1 yarns having 3.5 TM and are used asfilling yarns.

(e) A control yarn is produced from the untreated, scoured, and bleachedrawstock from which the treated blends are made, and it, too, is spuninto 13.5/1 yarn with a 3.5 TM and is used as filling yarns.

Weaving is carried out on a standard cotton loom at the rate of 165picks per minute, producing fabrics having 126 ends per inch and 50picks per inch (126 x 50). In this manner, fabrics made from the yarnsproduced from blends A, B, C, and the untreated control yarns, and theresulting fabrics contain a warp which is composed of 50% treated and50% untreated cotton fibers, the treated portion of which has a chemicaladd-on of 10.4% thermosetting resin. The fillings in each case containtreated fibers in the amount of 50% for Blend A, 25 for Blend B, and 75for Blend C, and the chemical add-on of the treated fiber portion is10.4%. The control Em filling, of course, contains no chemically treateders.

(E) Simulated trouser legs, 11% inches long by 9% inches wide with a 1/8 inch cuff, are then made from the fabrics produced in (D) above, withthe crease for the trouser leg, in one case, running in the warpdirection, and, in another case, in the filling direction. Afterfabrication, the experimental sample trouser legs and cuffs are pressedon a commercial-type steam press with the steam on for four seconds,with head pressure of pounds steam, and a holding time of 11 seconds.Temperature of pressing is 320 F. Immediately following pressing, thesamples are placed in a gas-fired cabinettype oven and cured at 320 F.for eight minutes. All samples are then equilibrated for at least 24hours before any physical testing is done.

Performance evaluation of the fabrics from which the above simulatedtrouser legs were made are carried out using laboratory test equipment,such as the Stoll flex and fiat abrasion-tests, tear strength test, andothers. In addition, the cured trouser leg samples are subjected to 40wash-tumble dry cycles in a commercially available home-type washingmachine and a commercially manufactured home-type electric dryer, eachof which meets the AATCC test method 88A 1964T. Each four-pound batch ofthese samples is washed with 75 cc. of a commercial detergent in eachwash cycle along with high water level. The washing period is eightminutes and is followed by a cold rinse and spin dry. The tumble dryingcycle requires 60 minutes. The test results with regard to abrasiondamage on these samples were extremely good. The following generalizedobservations can be made for the samples containing blends of treatedand untreated cotton fibers in both warp and filling:

(a) The crease retention in the leg portion of the samples was gas,regardless of the direction in which the pattern was cut.

(b) The cuff appearance (crease and shape retention) was good,regardless of the direction in which the pattern was cut.

No pilling was observed on the samples at any of the levels of add-onevaluated, nor at any of the percentages of treated fibers considered.

(d) Flat drying properties were good regardless of the direction inwhich the pattern had been cut; however, the samples cut in the warpdirection exhibited some puckering of cuif bottoms after five launderingcycles.

(e) Some seam pucker was noted in samples cut in the filling direction,while no seam pucker was noted in the samples cut in the conventionalwarp direction.

(f) More wear, due to abrasive damage, was apparent in samples that hadbeen cut in the conventional warp direction than in the samples that hadbeen cut in the transverse or filling direction. Very few of the samplesshowed any abrasive damage prior to the 30th washtumble dry cycle.

(g) About 2% shrinkage was observed in the conventional Warp directionsamples. This shrinkage occurred in both the warp and filling directionsof the fabric.

(h) Physical test data based on laboratory tests were as follows:

hours before use. Chemical add-on of this fabric calculated fromnitrogen determination was 8.34%.

For fabric FC.The treating solution contains:

6.25% dimethylol dihydroxy ethyleneurea, 0.25% alkylaryl polyglycol,3.75% ethyl alcohol, 0.35% zinc nitrate complex catalyst, 1% red dye,and 88.40% water. From the second nip, the fabric was passed through atender and dried at 185 F. to approximately 12% moisture content, thenequilibrated for 24 hours prior to use. The chemical add-on of thisfabric calculated from a nitrogen determination was 6.80%.

For fabric FD.-The treating solution consisted of z 5% dimethyloldihydroxy ethyleneurea, 0.25% alkylaryl polyglycol, 3.75% ethyl acohol,0.30% zinc nitrate complex catalyst, 1% dark red dye, and 89.70% water.From the final nip, the fabric was passed through a tenter and dried at185 F. to a moisture content of approximtaely 12%, then equilibrated for24 hours before use. Chemical add-on of this fabric calculated from anitrogen determination was 5.70%

For fabric FE.-The treating solution consisted of 3.75% dimethyloldihydroxy ethyleneurea, 0.25% alkylaryl polyglycol, 3.75 ethyl alcohol,0.25 zinc nitrate nitrate complex catalyst, 1% orange dye, and 91.00%water. From the final nip, the fabric passed through a tender and wasdried at 185 F. to a moisture content of about 12%, then equilibratedfor 24 hours before use. The chemical add-on of this fabric calculatedfrom a nitrogen determination was 4.39%.

In a manner parallel to that used in Example 4, simulated pants legs andcuffs (11% by 9 /8 with 1% cuffs) were made, and then pressed under thesame conditions as in Example 4, and then cured under the same Flexabrasion Tearing (grams) Wrinkle Resin, wt. Recovery percent Warp FillFlat abrasion Warp Fill Warp+Fill 1 Sample containing treated warp-l-Blend A in filling 5. 5 721 304 359 1, 967 l, 767 255 Sample containingtreated warp+ Blend B in filling 4.3 789 1,122 394 1, 700 567 2-19Sample containing treated warp+ Blend C 1n filling 6. 6 668 89 336 1,767 1, 400 267 Sample containing untreated warp and untreated filling983 1, 607 551 2, 833 3, 833 194 Sample containing treatedwarp-I-untreated filling 3. 4 794 1, 428 337 1, 533 3, 867 236 1 Awarp-l-fill angle of 240 is considered satisfactory for wash-wearfabrics.

Example 5 In this example, the performance characteristics of fivefabrics, impregnated with the same crosslinking agent by theconventional padding procedure, are compared with the fabrics of Example4. In this example, a 3/2 twill is made which contains scoured andbleached filling, and scoured and bleached warp yarns.

The fabrics are subjected to a padding operation consisting of two dipsand two nips in a pilot-scale padder with the final squeeze rollpressure adjusted to give a product having about 80% wet add-on.

For fabric FA.-The treating solution bath contains:

10% dimethylol dhydroxy ethyleneurea, 0.25 alkylaryl polyglycol, 3.75%ethyl alcohol, 0.5% zinc nitrate complex catalyst, 1% scarlet dye, and84.50% water. From the final nip, the fabric was passed through a tenderand dried at 185 F. to approximately 12% moisture content, thenequilibrated for 24 hours before use. Chemical add-on calculated fromnitrogen analysis was 9.55%.

For fabric FB.-The treating solution contains:

8.25% dimethylol dihydroxy ethyleneurea by weight, 0.25 alkylarylpolyglycol, 3.75 ethyl alcohol, 0.45% zinc nitrate complex catalyst, 1%turquoise dye, and 86.75% Water. From the final nip, the fabric waspassed through a tenter frame and dried at 185 F. to approximately 12%moisture content, then equilibrated for 24 conditions as used in Example4, and allowed to equilibrate for a minimum of 24 hours before testing,

Performance evaluation was made of these samples within the same laundrybatches as the samples produced in Example 4, and correspondinglaboratory determinations on flex and flat abrasion, tearing strength,and Monsanto wrinkle resistance were made on the fabrics from which thesimulated pants legs were made.

The following are generalized observations of the samples:

(a) Crease retention in the leg portion is equally good regardless ofthe direction in which the pattern was cut.

(b) The cuff appearance (crease and shape retention) is good regardlessof the direction in which the pattern was cut.

(c) No pilling is apparent on the samples at any of the chemical add-onlevels studied.

(d) Flat drying properties are good regardless of the direction in whichthe pattern was cut.

(e) Very little seam pucker is noted on the samples.

(f) Abrasive damage is apparent on all samples after as few as sevenlaundering and tumble-drying cycles. The samples had completely wornthrough in spots at the leg crease after as 10 laundering tumble-drycycles, and the cuffs exhibited holes at the top and bottom of 17 thecrease after as few as eight laundering tumble-dry cycles.

(g) Less than 2% shrinkage is observed regardless of the direction inwhich the pattern had been cut.

(h) Physical test data based upon laboratory tests were as follows:

ing resin selected from the group consisting of thermosetting resins anda mixture of thermosetting and thermoplastic resins to obtain a wetpick-up of about from 85 to 110 weight percent based on the weight ofthe cellulosic fiber;

(b) drying the resin-treated fiber from step (a) at a Flex abrasionTearing strength (grams) Wrinkle Resin, wt. recovery Sample Fabricpercent Warp Fill Flat abraslon Warp Fill Warp+Fill 1 1 A warp+fillangle of 240 is considered satisfactory for wash-wear.

Example 6 In the following example, data from Examples 5 and 6 areconsidered to show the improvement in flex abrasion and tearing strengthin fabrics produced from yarns containing blends of crosslinked fibersand untreated fibers when compared with fabrics containing similarquantities of crosslinking agents applied by present conventionalprocesses wherem the entire fabric 18 impregnated. and

Resin add-on Flex abrasion Tearing Str. (grams) Wrinkle wt. percentrecovery 2 to Warp Filling Warp Filling W-l-F Sample containing treatedwarp +Blend C in filling from Example 5 6. 6 668 89 l, 767 1, 400 267Fabric FOExample 6 6. 8 24 74 933 1, 183 280 Sample containing treatedwarp+B1end B in filling from Example 5 4. 3 78) 1, 122 1, 700 2, 567 249Fabric FE-Example 6.. 4. 4 233 l, 200 1, 900 263 Sample containingtreated warp+Blend A in filling from Example 5 5. 5 721 304 l, 967 1,767 255 Fabric 1 DExamp1e 6 5. 7 19 46 933 l, 233 287 l Resin add-on wasdetermined by nitrogen analysis.

A warp +filling wrinkle recovery angle of 240 is considered satisfactorywash-wear fabrics.

It will be observed that in all cases there is a sharp reduction in flexabrasion and tearing strength for the same resin add-on where the fabricis treated by conventional padding processes.

We claim:

1. A process for producing yarn from a blend of untreated cellulosicfiber and resin-treated cellulosic fiber in which resin-treated fiberthe resin has not been cured, comprising (a) treating cellulosic fiberwith an aqueous solution of a catalyst and an essentially monomericcrosslinking resin selected from the group consisting of thermosettingresins and a mixture of thermosetting and thermoplastic resins to obtaina wet pick-up of about from 85 to 110 weight percent based on the weightof the cellulosic fiber;

(b) drying the resin-treated fiber from step (a) at a temperature belowabout 200 F. to obtain uncured, resin-treated cellulosic fiber at anequilibrated moisture content of about from 5.5 to 8.0 weight percentbased on the total weight of the fiber and deposited resin;

(c) blending the dried, uncured, resin-treated cellulosic fiber fromstep (b) with untreated cellulosic fibers; and

(d) forming yarn from the blended fiber of step (c).

2. The process of claim 1 wherein the crosslinking resin is athermosetting resin.

3. The process of claim 1 wherein the crosslinking resin is a mixture ofthermosetting and thermoplastic resins.

4. A process for producing a crosslinked cellulosic yarn from a blend ofuntreated cellulosic fiber and resintreated cellulosic fiber in whichresin-treated fiber the resin has not been cured, comprising (a)treating cellulosic fiber with an aqueous solution of a catalyst and anessentially monomeric crosslink- (e) curing the crosslinking resin inthe yarn from step (d) at a temperature of about from 240 F. to 350 F.using curing times of about from 20 to 3 minutes.

5. The process of claim 4 wherein the crosslinking resin is athermosettingresin.

6. The process of claim 4 wherein the crosslinking resin is a mixture ofthermosetting and thermoplastic resins.

7. A process for preparing a wash-wear cellulosic fabric from a blend ofuntreated cellulosic fiber and resintreated cellulosic fiber wherein theresin treated moiety has not been cured to induce crosslinking,comprising (a) forming a fabric from yarn produced by the process ofclaim 1; and

(b) curing the fabric formed in step (a) to induce a crosslinkingreaction.

8. The process of claim 7 wherein the crosslinking resin used is athermosetting resin.

9. The process of claim 7 wherein the crosslinking resin used is amixture of thermosetting and thermoplastic resins.

10. A process for preparing a wash-wear garment from a cellulosic fabriccomposed of a blend of untreated cellulosic fiber and resin-treatedcellulosic fiber wherein the resin-treated moiety has not been cured toinduce crosslinking, comprising (a) forming a fabric from yarn producedby the process of claim 1;

(b) forming a garment from the fabric of step (a); and

(c) curing the garment formed in step (b) to induce a crosslinkingreaction.

11. The process of claim 10 wherein the crosslinking resin used is athermosetting resin.

12. The process of claim 10 wherein the crosslinking resin used is amixture of thermosetting and thermoplastic resins.

(References on following page) 3,483,570 1 9 References Cited UNITEDSTATES PATENTS 20 GEORGE F. LESMES, Primary Examiner J. CANNON,Assistant Examiner 5/1938 Bowen et a1.

11/1961 Pitts 57 153 X CL 4/1964 Brown 6161 57164 5 8115.6, 116.3;28-75; 38-444; 57-140; 153, 156, 11/1965 Lund et al.

